铂基氧还原电催化剂的结构演变

doi:10.1016/S1872-2067(21)63896-2

催化学报 ›› 2022, Vol. 43 ›› Issue (1): 47-58.DOI: 10.1016/S1872-2067(21)63896-2

铂基氧还原电催化剂的结构演变

彭佳恒^a, 陶鹏^a, 宋成轶^a, 尚文^a, 邓涛^a^,^b, 邬剑波^a^,^b^,^c^,^d^,^*()

^a上海交通大学材料科学与工程学院金属基复合材料国家重点实验室, 上海200240
^b上海交通大学氢科学中心, 上海200240
^c上海交通大学材料基因组联合研究中心, 上海200240
^d上海交通大学张江高研院未来材料创制中心, 上海200240

收稿日期:2021-05-30 接受日期:2021-06-15 出版日期:2022-01-18 发布日期:2021-11-15
通讯作者: 邬剑波
基金资助:
国家重点研发计划(2017YFB0406000);国家自然科学基金(21875137);国家自然科学基金(51521004);国家自然科学基金(51420105009);111项目(B16032);上海市教委创新计划项目(2019-01-07-00-02-E00069);上海交通大学氢科学中心资助

Structural evolution of Pt-based oxygen reduction reaction electrocatalysts

Jiaheng Peng^a, Peng Tao^a, Chengyi Song^a, Wen Shang^a, Tao Deng^a^,^b, Jianbo Wu^a^,^b^,^c^,^d^,^*()

^aState Key Laboratory of Metal Matrix Composites, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
^bCenter of Hydrogen Science, Shanghai Jiao Tong University, Shanghai 200240, China
^cMaterials Genome Initiative Center, Shanghai Jiao Tong University, Shanghai 200240, China
^dFuture Material Innovation Center, Zhangjiang Institute for Advanced Study, Shanghai Jiao Tong University, Shanghai 200240, China

Received:2021-05-30 Accepted:2021-06-15 Online:2022-01-18 Published:2021-11-15
Contact: Jianbo Wu
About author:* Tel/Fax: +86-21-54745582; E-mail: jianbowu@sjtu.edu.cn
Supported by:
National Key R&D Program of China(2017YFB0406000);National Natural Science Foundation of China(21875137);National Natural Science Foundation of China(51521004);National Natural Science Foundation of China(51420105009);111 Project(B16032);Innovation Program of Shanghai Municipal Education Commission(2019-01-07-00-02-E00069);fund from Center of Hydrogen Science and Joint Research Center for Clean Energy Materials

摘要/Abstract

摘要：

质子交换膜燃料电池的商业化有望在不久的将来实现更清洁的能源社会. 然而, 氧还原反应缓慢的反应动力学和苛刻的条件对质子交换膜燃料电池的寿命和成本产生了巨大的挑战. 之前大多数铂基催化剂的设计都将重点更多地放在提高活性上. 随着质子交换膜燃料电池的商业化, 寿命问题也受到了更多的关注. 对整个生命周期中结构演变进行深入地了解, 有助于优化铂基催化剂的活性和寿命. 原位电子显微表征以及其他原位技术的发展推动了对演变机理的揭示. 本文着重介绍了铂基催化剂在结构演变方面的最新进展, 具体包括催化剂合成、后处理以及电催化过程中的结构演变. 本文所涉及的结构演变主要包含四组, 分别是溶解与浸出、奥斯瓦尔德熟化与合并、偏析以及相变. 此外, 本文还列出了未来铂基氧还原电催化剂结构演变研究面临的一些挑战.
铂溶解是铂基催化剂失效的主要原因之一. 甫尔拜图显示了铂热力学稳定相的转化关系, 但是实际溶解过程中受到复杂的动力学因素影响. 铂溶解机理主要包括铂的直接电溶解和铂氧化物的化学溶解. 在电化学老化过程中, 铂的溶解往往伴随着晶面的粗化. 铂溶解受到很多因素(包括尺寸、晶面以及微量的杂质等)的影响. 合金化能够提高铂基催化剂的活性, 但同时伴随着合金元素快速浸出的问题, 这种现象在三电极体系以及实际燃料电池运行过程中都非常显著. 核壳催化剂能够进一步提高铂的活性和利用率, 但需要对核进行保护. 利用脱合金可以制备具有更大电化学活性面积的催化剂, 对燃料电池大功率运行时的性能更加有利. 奥斯瓦尔德熟化和合并导致铂基催化剂的长大, 在电催化以及热处理过程中导致催化剂性能的损失. 燃料电池实际工况中碳腐蚀会加速合并, 因此耐腐蚀的载体能够有效提高催化剂的稳定性. 富过渡金属元素的低铂催化剂在热处理中更容易发生合并. 然而不利的催化剂熟化和合并也提供了无表面活性剂合成高性能铂基催化剂的有效途径. 在晶体生长、后处理以及电催化过程中都会发生元素偏析, 通过控制热处理的气氛, 可以实现元素分布的控制. 偏析的晶体脱合金后可以方便地得到纳米框架. 从无序合金到金属间化合物的转变能够同时提高催化剂的活性和稳定性, 受到了广泛的关注. 但是有序化转变需要较高的温度, 往往会造成严重的烧结. 相比高温直接转变, 低温扩散预处理能够降低有序化转变温度, 但是会造成催化剂球化.
对于未来铂基氧还原电催化剂结构演变的研究, 仍存在挑战. 首先, 更深入地了解结构演化需要具有更高时空分辨率甚至达到原子尺度的先进原位表征技术. 其次, 液相光电子能谱的开发可能是研究电催化过程中表面羟基/氧化物演化的一种具有前景的方法. 此外, 还需要努力建立结构演化过程中性能和结构之间的实时对应关系, 从而区分出最优的中间结构. 随后的挑战是保持催化剂的最佳结构. 此外, 还需要进一步探索更全面的避免不利演变和促进有利演变的策略.

关键词: 氧还原反应, 结构演变, 铂基催化剂, 寿命, 原位电子显微表征

Abstract:

The commercialization of proton exchange membrane fuel cells (PEMFCs) could provide a cleaner energy society in the near future. However, the sluggish reaction kinetics and harsh conditions of the oxygen reduction reaction affect the durability and cost of PEMFCs. Most previous reports on Pt-based electrocatalyst designs have focused more on improving their activity; however, with the commercialization of PEMFCs, durability has received increasing attention. In-depth insight into the structural evolution of Pt-based electrocatalysts throughout their lifecycle can contribute to further optimization of their activity and durability. The development of in situ electron microscopy and other in situ techniques has promoted the elucidation of the evolution mechanism. This mini review highlights recent advances in the structural evolution of Pt-based electrocatalysts. The mechanisms are adequately discussed, and some methods to inhibit or exploit the structural evolution of the catalysts are also briefly reviewed.

Key words: Oxygen reduction reaction, Structural evolution, Pt-based electrocatalyst, Durability, In situ electron microscopy, characterizations

彭佳恒, 陶鹏, 宋成轶, 尚文, 邓涛, 邬剑波. 铂基氧还原电催化剂的结构演变[J]. 催化学报, 2022, 43(1): 47-58.

Jiaheng Peng, Peng Tao, Chengyi Song, Wen Shang, Tao Deng, Jianbo Wu. Structural evolution of Pt-based oxygen reduction reaction electrocatalysts[J]. Chinese Journal of Catalysis, 2022, 43(1): 47-58.

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图/表 11

Fig. 1. (A) Pourbaix diagram of Pt(100); (B) CV spectra and corresponding dissolution amount of Pt(110), Pt(100), and Pt(111); (C) Graphical representation of the main reactions that occur at the Pt electrodes (pH = 1). Reprinted with permission from: (A) Ref. [7], copyright 2018, American Chemical Society and (B) Ref. [9], Copyright 2016, American Chemical Society.

Fig. 2. (A) CV spectra and in situ STM images of Pt(111); (B) Depiction of the surface roughing mechanism; (C) STM images of Pt(111) after different protocols. Reprinted with permission from: (A,B) Ref. [15], copyright 2017, American Chemical Society and (C) Ref. [14], Copyright 2018, Elsevier.

Fig. 3. (A) Sequential TEM images of the icosahedral and cubic Pt NPs; (B) Plots for the oxidative etching of the icosahedral Pt NPs at different stages of the reaction. (C) Analysis of the etching modes of the different sites on a cubic Pt NP. Reprinted with permission from Ref. [18], Copyright 2017, American Chemical Society.

Fig. 4. (A) TEM images; (B) Schematic of the etching process; (C) Strain map before etching; (D) Etching distance in the three directions; (E) Etching rates in the three directions. Reprinted with permission from Ref. [32], Copyright 2020, Elsevier.

Fig. 5. (A) Scheme of the synthesis of the Pt-Ir-Pd nanocages; (B) HAADF-STEM image and EDX maps of the Pt-Ir-Pd nanocage; (C) Scheme of the synthesis of porous Pt3Ni NWs; (D) TEM and HAADF-STEM images of the Pt3Ni6 NWs; (E) TEM and HAADF-STEM images of the porous treated Pt3Ni6 NWs. Reprinted with permission from: (A,B) Ref. [40], Copyright 2020, Wiley-VCH and (C-E) Ref. [42], Copyright 2017, Wiley-VCH.

Fig. 6. (A) Indirect nanoplasmonic sensing centroid shift vs. time in Ar at 453 K for Pt clusters with different size distributions; (B) Cluster area distribution before and after annealing. Reprinted with permission from Ref. [49], Copyright 2014, American Chemical Society.

Fig. 7. (A-C) HAADF-STEM images of PtM3/C; (D,E) STEM-EELS mapping of the PtCo3 and PtNi3 NPs; (F) Surface composition determined by XPS; (G,H) Structure models of (D) and (E); (I) Ni content and particle size of the PtNi3 NPs at 400 and 600 °C; (J) Scheme of the surface composition effect on coalescence. Reprinted with permission from ref. [56], Copyright 2020, American Chemical Society.

Fig. 8. (A) Scheme of the Pt NW formation process in the presence of H2; (B) TEM images of the growth process; (C) TEM images of oriented attachment growth along the Pt(100) facet. Reprinted with permission from Ref. [69], Copyright 2017, Wiley-VCH.

Fig. 9. (A,B) XANES spectra of the PtCo/C electrocatalyst at the Co K-edge before and after ADT using different potentials; (C-F) STEM images of an oxidized Pt3Co NP; (G,H) Bright-field STEM images of an oxidized Pt3Co NP. Reprinted with permission from: (A,B) Ref. [11], Copyright 2019, American Chemical Society; (C)-(H) Ref. [78], Copyright 2017, American Chemical Society.

Fig. 10. (A) Schematic diagram of the formation of phase-segregated octahedral PtNi NPs; (B-E) Elemental maps of the PtNi NPs during the synthesis process; (F-H) HAADF-STEM images of the phase-segregated hierarchical PtNi NPs and their derivatives produced by chemical etching; (I) EDX elemental maps of the octahedral skeletal Pt-based NPs. Reprinted with permission from Ref. [81], Copyright 2015, American Chemical Society.

Fig. 11. (A-D) HAADF-STEM images along the (100) surface; (E-H) HAADF-STEM images along the (110) surface; (I) Scheme of the evolution process of the Pt3Co NCs under LTDAP and DHTAP. Reprinted with permission from Ref. [88]. Copyright 2021, American Chemical Society.

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铂基氧还原电催化剂的结构演变

Structural evolution of Pt-based oxygen reduction reaction electrocatalysts

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